锥面玻碳旋转电极研制及在尿铅测定中的应用

发布时间：2018-06-26 09:40

本文选题：锥面玻碳旋转电极 + 溶出分析　；参考：《齐齐哈尔大学》2012年硕士论文

【摘要】：玻碳电极作为一种电分析化学中重要的极谱电极，具有导电性好，化学稳定性高，热胀系数小，质地坚硬，气密性好，电势适用范围宽，电极形状多样等特点。用它作基体还可制成汞膜玻碳电极和化学修饰电极等，广泛应用于微量元素的测定中。因此新型玻碳电极的研制具有较高的应用价值和广阔的应用前景。本工作提出了一种改进的锥面玻碳电极设计。用AutoCAD对各部件进行设计，并进行零件加工和组装。经过改进的用于溶出分析的锥面玻碳旋转电极及微型电解池，具有死体积小，传质速率高、不受微管路中微小气泡影响，使溶液在玻碳电极斜面产生较强的冲击力且不吸附氢气。采用双碳触点引导电流和冲富集消除金属间化合物的干扰，程控泵实现在线更换底液。本工作使用PS4.0极谱溶出仪，采用电位溶出内标分析法测定了尿液中的铅含量。实现了一次测量就可得到尿液中铅含量，校正比例系数使尿铅浓度值与峰高值相等(Cx=Hx)。减少了工作曲线法和标准加入法测定尿铅的复杂性。在测量溶液中加入10.00μg/镉（II）作为内标物,线性回归方程为C(μg/L)=-1.01354+1.46Hp,相关系数r=0.99,相对校正系数F=1.46。铅的一阶导数溶出峰高与铅浓度在0～80μg/L之间呈线性关系，测量结束后将内标物峰高校正146.58，，提高了铅测量的精度。尿液标本在电解池中直接进行电位溶出测定。平均回收率为104%～115.98%，测量铅含量为63.48μg/L的标样，测量值63.76μg/L，相对标准偏差RSD=0.44%。结果表明，用内标法测定尿液中铅含量操作简单，有较好的灵敏性和准确性。
[Abstract]:As an important polarographic electrode in electroanalytical chemistry, glassy carbon electrode is characterized by good electrical conductivity, high chemical stability, small thermal expansion coefficient, hard texture, good airtightness, wide potential application range and various electrode shapes. The glassy carbon electrode with mercury film and chemically modified electrode can be made by using it as substrate. It is widely used in the determination of trace elements. Therefore, the development of new glassy carbon electrode has high application value and broad application prospect. In this work, an improved design of cone glassy carbon electrode is presented. The parts are designed by AutoCAD, and the parts are processed and assembled. The improved cone surface glassy carbon rotating electrode and miniature electrolytic cell for dissolution analysis have small dead volume, high mass transfer rate and are not affected by micro bubbles in the microtube. The solution has a strong impact force on the glassy carbon electrode slope and does not adsorb hydrogen. The intermetallic compound interference is eliminated by double carbon contact guiding current and flushing enrichment, and the on-line replacement of substrate solution is realized by program-controlled pump. In this work, the content of lead in urine was determined by potentiometric stripping internal standard method with PS4.0 polarographic stripping apparatus. The lead content in urine can be obtained by a single measurement, and the correction ratio coefficient makes the concentration of lead in urine equal to the peak value (CxX Hx). The complexity of working curve method and standard addition method for determination of lead in urine is reduced. 10.00 渭 g / CD (II) was added as the internal standard. The linear regression equation was C (渭 g / L) -1.01354 1.46 Hp, the correlation coefficient was 0.99, and the relative correction coefficient was F1.46. There is a linear relationship between the peak height of the first derivative dissolution of lead and the lead concentration in the range of 0 ~ 80 渭 g / L. After the measurement, the internal standard peak is 146.58, which improves the precision of lead measurement. Urine samples were directly determined by potentiometric dissolution in the electrolytic cell. The average recovery was 104 and 115.98, the lead content was 63.48 渭 g / L, the measured value was 63.76 渭 g / L, the relative standard deviation (RSD) was 0.44%. The results showed that the determination of lead in urine by internal standard method was simple, sensitive and accurate.
【学位授予单位】：齐齐哈尔大学
【学位级别】：硕士
【学位授予年份】：2012
【分类号】：R131;O657.1

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